US4469663A - Scale control in flue gas desulfurization - Google Patents

Scale control in flue gas desulfurization Download PDF

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Publication number
US4469663A
US4469663A US06/434,676 US43467682A US4469663A US 4469663 A US4469663 A US 4469663A US 43467682 A US43467682 A US 43467682A US 4469663 A US4469663 A US 4469663A
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United States
Prior art keywords
solution
gas
slurry
sulfur oxides
contacting
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Expired - Fee Related
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US06/434,676
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English (en)
Inventor
Druce K. Crump
David A. Wilson
Gary D. Gatton
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Dow Chemical Co
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Dow Chemical Co
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Priority to US06/434,676 priority Critical patent/US4469663A/en
Assigned to DOW CHEMICAL COMPANY THE reassignment DOW CHEMICAL COMPANY THE ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: CRUMP, DRUCE K., GATTON, GARY D., WILSON, DAVID A.
Priority to CA000461337A priority patent/CA1215822A/en
Priority to EP84305723A priority patent/EP0172288B1/en
Priority to AU32597/84A priority patent/AU573617B2/en
Priority to JP59182917A priority patent/JPS6161617A/ja
Application granted granted Critical
Priority to IN675/MAS/84A priority patent/IN161736B/en
Publication of US4469663A publication Critical patent/US4469663A/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
    • C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
    • C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
    • C02F5/14—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing phosphorus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/50—Sulfur oxides
    • B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/50—Sulfur oxides
    • B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
    • B01D53/502—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound characterised by a specific solution or suspension

Definitions

  • the present invention provides just such a method.
  • Particular methylenephosphonates have been discovered which will keep the metal ions in solution during the contacting phase and allow precipitation in a subsequent step.
  • Certain heterocyclic amine polymers which have been methylenephosphonated have been found to be particularly useful in a flue gas desulfurization process in which the subject polymers act as threshold agents in the control of metal ions in the gas-contacting step of the process, but allow subsequent precipitation of these ions as sulfates in a later step.
  • polymeric methylenephosphonated amines primarily dimers and trimers of aminoethylpiperazine (AEP)
  • AEP aminoethylpiperazine
  • A is an organic radical having the formula ##STR1## wherein F is hydrogen, hydroxyethyl, hydroxypropyl, ##STR2## wherein M is hydrogen, an alkali metal or ammonium, and wherein B is a divalent radical derived from a dihalo or haloepoxy organic compound having one of the following structures ##STR3## and wherein n is 1 to 10; n' is 1 to 3; R is hydrogen or methyl; and m is 1 to 10 and at least 50% of the F groups are ##STR4##
  • the threshold active compounds of the invention are effective in preventing precipitation of metal ions, e.g. Ca ++ as scale, when water soluble compounds containing these metals are employed in aqueous scrubbing solutions employed to scrub sulfur oxides from flue gas from the burning of sulfur-containing hydrocarbon fuels.
  • the amount of threshold agent i.e. the phosphonomethylated AEP polymeric products, usually employed is from about 0.5 to about 500 ppm depending upon the particular agent and upon the amount of metal ions present in solution, which in turn depends upon the volume of gas and concentration of sulfur oxides therein.
  • the FIGURE is a schematic diagram of a typical absorber tower and associated equipment employed in a gas desulfurization process.
  • an absorbent tower 10 and a feed tank 11.
  • stirring means 23 driven by motor m.
  • absorber tower 10 is packed section 21 for contacting gas and liquid, and a second packed section 22 for demisting the gas prior to exiting outlet pipe 27.
  • the gas to be desulfurized enters the tower 10 through inlet pipe 26.
  • Conduits 31 and 33 for circulating liquid lead from feed tank 11 to absorber tower 10 and conduit 35 for recirculating liquid from quench sump 51 leads to tower 10; liquid distributor means, e.g. spray nozzles 41, 42, 43 and 44 are connected to conduits 31, 37, 33 and 35, respectively.
  • Distributor means 41 and 43 conduct absorbing solution (slurry) to packed section 21 and into collector 52 in order to contact the gas coming into tower 10 via pipe 26.
  • Distributor means 42 conducts water into packed section 22 to remove particulate moisture from the upwardly flowing gas prior to its exit via pipe 27.
  • Distributor means 44 sprays a slurry from quench sump 51 which contacts and cools gas entering the bottom of the column through pipe 26.
  • Conduit 38 is an overflow pipe to the feed tank which leads to the quench sump 51.
  • Collector 52 carries substantially all of the absorbing liquid admitted to tower 10 via conduits 31 and 33 and returns it to feed tank 11 via conduit 34.
  • An overflow conduit 38 permits replenishment of the quench sump 51 from feed tank 11 as needed when portions of the quench sump bottoms are sent to a thickener (not shown) via conduit 36. Pumps in the system are indicated by the letter p.
  • the threshold agent of the present invention is added to the aqueous feed in tank 11 or into the feed in conduit pipes 31 and 33 at a point just prior to their entrance into tower 10.
  • the aqueous solution and/or slurry of CaCO 3 is fed into the upper portion of tower 10 from feed tank 11 via conduits 31 and 33 and through distributors 41 and 43.
  • the gas stream to be desulfurized enters tower 10 at its lower end through pipe 26 at a temperature of about 85° C. where it first contacts quench liquid from quench sump 51 which is pumped via conduit 35 to distributor 44.
  • the temperature achieved during the contacting step in the upper portion of the tower is normally 55°-60° C. while the temperature in the quench sump is typically 70°-80° C.
  • An ideal inhibitor should prevent deposition in the packed (contact) section of the tower but allow precipitation to occur in the sump.
  • a packed column was connected at its upper and lower ends by tubing to a vessel containing a supersaturated solution of calcium sulfate (initial pH 3.5-4). This solution was circulated through the column by introducing the said solution at its upper end and returning it through the tubing connecting its lower end to the said vessel.
  • the column was packed with pieces of polyethylene tubing, 0.375" long ⁇ 0.375" diameter (0.95 cm ⁇ 0.95 cm).
  • Precipitation of calcium sulfate scale on the packing was noted with time and calcium remaining in solution was determined by filtering a sample of the solution through a millipore filter and titrating with standard disodium ethylenediaminetetraacetate. While circulating at a temperature of 54° C. without any scale inhibitor, nearly half the calcium sulfate present had precipitated, forming scale, within 30 minutes to one hour. The amount of CaSO 4 present in solution at the start of the test was 3985 ppm, after 30 minutes circulation only 2162 ppm remained and 2067* ppm after 70 minutes.
  • EOC ethylene dichloride
  • reaction product was then phosphonomethylated by adding approximately 75 g of concentrated hydrochloric acid and 32.6 g (0.40 mole) of phosphorous acid to the aqueous amine solution and the reaction mixture heated to reflux and maintained for one hour.
  • Aqueous 37% formaldehyde solution, 28.1 g (0.35 mole) was added through the addition funnel over a one and one-half hour period.
  • the reaction mixture was heated at reflux for an additional three hours and then cooled.
  • the product was evaluated by employing it in the laboratory circulating apparatus described above.
  • Example 1 The product of Example 1 was evaluated in the above-described test equipment at 10 ppm (active acid) at temperatures of 54° C., 75° C., and 90° C.
  • the data is summarized in Table I.
  • the data indicates the effectiveness of the EDC/AEP phosphonate inhibitor. It prevents deposition of scale at 54° C. (as in the contacting section) but then allows the calcium sulfate to precipitate on heating (as in the sump section).
  • a supersaturated solution of calcium sulfate was prepared containing 10 ppm of aminotrimethylenephosphonic acid (ATMPA), a commercially available organophosphonic acid inhibitor.
  • ATMPA aminotrimethylenephosphonic acid
  • the solution was circulated at 54° C. and titrated periodically for soluble calcium. The same thing was done, but employing a commercially available aminomethylenephosphonic acid, diethylenetriaminepentamethylenephosphonic acid (DETA-MPA), again at 10 ppm based on the weight of solution.
  • DETA-MPA diethylenetriaminepentamethylenephosphonic acid
  • Aminoethylpiperazine the compound from which the methylenephosphonate of the present invention is made, was reacted with formaldehyde and phosphorous acid to make its trimethylenephosphonic acid derivative. This was used at 10 ppm (active acid) as in Comparative Example A. Little, if any, calcium sulfate scale was observed on the packing at either 54° or 75° C. As in Comparative Example A, the aminoethylpiperazinetrimethylenephosphonic acid inhibitor is not suited for use in the desulfurization unit since it would not allow the calcium sulfate to precipitate at 75° C., but kept it in solution at both temperatures.
  • An aminoethylpiperazine derived amine was prepared by reacting aminoethylpiperazine and ethylenedichloride in an EDC/AEP mole ratio of 0.80.
  • the product was phosphonomethylated with phosphorous acid and formaldehyde in the presence of hydrochloric acid to give the methylenephosphonic acid derivative.
  • the product was evaluated at 10 ppm (active acid) at temperatures of 54° C. and 75° C. as in Example 2. Results are shown in Table III.
  • the compounds that have been shown to be effective in the process are methylenephosphonic acids derived from the phosphonomethylation of aminoethylpiperazine-ethylenedichloride reaction products.
  • acid derivatives themselves various metal and alkali metal salts; ammonium and amine salts; partial salts of the methylenephosphonic acids; and mixtures thereof can be employed.
  • the preferred products are those that have had the aminohydrogens fully replaced by methylenephosphonic acid groups. However, some aminohydrogens can be left unreacted if desired. Also, functionality in addition to the methylenephosphonic acid group can be incorporated into the compounds. Typical groups are hydroxyalkyl, methylenesulfonate, hydroxypropylsulfonate, carboxymethyl, etc.
  • alkylene dihalides which may be saturated or unsaturated, aralkylene dihalides or dihalo ethers, and epoxyhalides, such as epichlorohydrin, can be used to react AEP to prepare the amines which are then phosphonomethylated.
  • the present invention is an improvement in the process of gas desulfurization in which the gas is contacted with an aqueous solution or slurry of a calcium salt or hydroxide to remove the sulfur oxides contained therein.
  • This contact causes the formation of calcium sulfate which precipitates as scale on the surfaces wherein the contact occurs.
  • the invention is to employ a particular threshold agent which will inhibit the scale formation on the contact surfaces, but permit it to occur in another part of the system.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Treating Waste Gases (AREA)
US06/434,676 1982-10-15 1982-10-15 Scale control in flue gas desulfurization Expired - Fee Related US4469663A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US06/434,676 US4469663A (en) 1982-10-15 1982-10-15 Scale control in flue gas desulfurization
CA000461337A CA1215822A (en) 1982-10-15 1984-08-20 Scale control in flue gas desulfurization
EP84305723A EP0172288B1 (en) 1982-10-15 1984-08-22 The use of polymeric alkylenephosphoric acid piperazine derivatives for scale control in flue gas desulfurization
AU32597/84A AU573617B2 (en) 1982-10-15 1984-08-31 Scale control in flue gas desulphurization
JP59182917A JPS6161617A (ja) 1982-10-15 1984-09-03 煙道ガス脱硫におけるスケ−ル制御用の重合状アルキレン燐酸ピペラジン誘導体
IN675/MAS/84A IN161736B (Sortimente) 1982-10-15 1984-09-04

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US06/434,676 US4469663A (en) 1982-10-15 1982-10-15 Scale control in flue gas desulfurization

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US (1) US4469663A (Sortimente)
EP (1) EP0172288B1 (Sortimente)
JP (1) JPS6161617A (Sortimente)
AU (1) AU573617B2 (Sortimente)
CA (1) CA1215822A (Sortimente)
IN (1) IN161736B (Sortimente)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4735787A (en) * 1987-08-17 1988-04-05 Nalco Chemical Company Scale inhibitor for intermittent washed mist eliminators in flue gas desulfurization systems
US4783327A (en) * 1987-08-13 1988-11-08 The Dow Chemical Company Sulfur dioxide removal from gas streams using hydroxyalkyl substituted piperazinones
US4786329A (en) * 1987-09-09 1988-11-22 The Dow Chemical Company Asphalt compositions containing anti-stripping additives prepared from amines or polyamines and phosphonates
US5077023A (en) * 1989-08-01 1991-12-31 Basf Aktiengesellschaft Reduction in the rate of oxidation of sulfite solutions
US5098681A (en) * 1990-08-16 1992-03-24 The Dow Chemical Company Process for absorption of sulfur compounds from fluids
US5108723A (en) * 1990-08-16 1992-04-28 The Dow Chemical Company Process for absorption of sulfur compounds from fluids
US5120516A (en) * 1990-01-08 1992-06-09 Physical Sciences, Inc. Process for removing nox emissions from combustion effluents
US5236678A (en) * 1990-08-16 1993-08-17 The Dow Chemical Company Process for absorption of sulfur compounds from fluids using piperidines
US5342593A (en) * 1990-08-16 1994-08-30 The Dow Chemical Company Process for absorption of sulfur compounds from fluids
US5433934A (en) * 1991-08-13 1995-07-18 The Dow Chemical Company Method for simultaneous absorption of sulfur dioxide and nitric oxide from flue gas
CN102580504A (zh) * 2012-03-07 2012-07-18 武汉兴能环保技术有限公司 一种新型氨法脱硫吸收装置
US20130220888A1 (en) * 2012-02-29 2013-08-29 Uop, Llc Process, vessel, and apparatus for removing one or more sulfur compounds

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI78846B (fi) * 1985-04-24 1989-06-30 Tampella Oy Ab Foerfarande foer avlaegsnande av gasformiga svavelfoereningar och svaveldioxid ur roekgaser i en panna.
PL279643A1 (en) * 1988-05-26 1990-01-22 Jednotne Zemedelske Druzstvo P Method of and apparatus for removing heavy hydrocarbons and their derivatives from gaseous mixtures
US5202103A (en) * 1991-12-20 1993-04-13 Union Carbide Chemicals & Plastics Technology Corporation Removal of sulfur dioxide from gas streams
DE10204818C2 (de) 2002-02-06 2003-11-27 Eurotope Entwicklungsgesellsch Gerät und Verfahren zur Beladung von Implantationshohlnadeln mit Strahlungsquellen aus Strahlungsquellenketten zur interstitiellen Brachytherapie von Gewebe
DE50307128D1 (de) * 2003-06-03 2007-06-06 Eckert & Ziegler Eurotope Gmbh Gerät und Verfahren zur Beladung von Implantationshohlnadeln mit Strahlungsquellen aus Strahlungsquellenketten zur interstitiellen Brachytherapie von Gewebe

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US3303139A (en) * 1962-01-27 1967-02-07 Henkel & Cie Gmbh Aminophosphonic acids and their derivatives as complex formers for metal ions
US3883639A (en) * 1971-08-12 1975-05-13 Pullman Inc Method of removing sulfur-containing gases from waste gas
US4003848A (en) * 1974-12-10 1977-01-18 Union Carbide Corporation Method for the adsorption of sulfur dioxide
US4100256A (en) * 1977-03-18 1978-07-11 The Dow Chemical Company Hydrolysis of carbon oxysulfide
US4118318A (en) * 1976-10-26 1978-10-03 Calgon Corporation Gas scrubber scale and deposit control
US4148615A (en) * 1974-12-30 1979-04-10 Kennecott Copper Corporation Prevention of scale formation in wet lime scrubbers
US4150096A (en) * 1977-10-31 1979-04-17 Nelms William M Process for treating combustion gases
US4171292A (en) * 1976-08-05 1979-10-16 Betz Laboratories, Inc. Compositions for treating aqueous mediums containing magnesium sulfite trihydrate
US4177245A (en) * 1978-05-24 1979-12-04 Battelle Development Corporation Scale suppression in lime and limestone scrubbers
US4213946A (en) * 1976-12-21 1980-07-22 Kobe Steel, Ltd. Process for preventing formation of gypsum scale in a flue gas desulfurization process
US4216087A (en) * 1978-12-18 1980-08-05 The Dow Chemical Company Scrubber scale prevention
US4310348A (en) * 1978-08-22 1982-01-12 Egyt Gyogyszervegyeszeti Gyar Plant growth regulating compositions
US4336233A (en) * 1975-11-18 1982-06-22 Basf Aktiengesellschaft Removal of CO2 and/or H2 S and/or COS from gases containing these constituents
US4388281A (en) * 1980-05-24 1983-06-14 Hoelter Heinz Noxious-component removal from flue gas and compositions useful therefor

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US3859211A (en) * 1968-10-17 1975-01-07 Petrolite Corp Water clarification with nitrogen-heterocyclic phosphonic acids
US3799893A (en) * 1971-03-31 1974-03-26 Petrolite Corp Methylene phosphonates of glycidyl reacted polyamines
SE435456B (sv) * 1976-01-07 1984-10-01 Calgon Corp Komposition och forfarande for att kontrollera uppbyggnaden av pannsten i gastvettare
US4138353A (en) * 1977-04-01 1979-02-06 The Mogul Corporation Corrosion inhibiting composition and process of using same
US4409192A (en) * 1982-04-26 1983-10-11 Betz Laboratories, Inc. Gas scrubbing methods
US4489203A (en) * 1982-09-27 1984-12-18 The Dow Chemical Company Polyumeric alkylene phosphoric acid piperazine derivatives as scale inhibitors
CA1207211A (en) * 1982-09-27 1986-07-08 Dionisio G. Cuisia Composition and method for inhibiting scale

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3303139A (en) * 1962-01-27 1967-02-07 Henkel & Cie Gmbh Aminophosphonic acids and their derivatives as complex formers for metal ions
US3883639A (en) * 1971-08-12 1975-05-13 Pullman Inc Method of removing sulfur-containing gases from waste gas
US4003848A (en) * 1974-12-10 1977-01-18 Union Carbide Corporation Method for the adsorption of sulfur dioxide
US4148615A (en) * 1974-12-30 1979-04-10 Kennecott Copper Corporation Prevention of scale formation in wet lime scrubbers
US4336233A (en) * 1975-11-18 1982-06-22 Basf Aktiengesellschaft Removal of CO2 and/or H2 S and/or COS from gases containing these constituents
US4171292A (en) * 1976-08-05 1979-10-16 Betz Laboratories, Inc. Compositions for treating aqueous mediums containing magnesium sulfite trihydrate
US4118318A (en) * 1976-10-26 1978-10-03 Calgon Corporation Gas scrubber scale and deposit control
US4213946A (en) * 1976-12-21 1980-07-22 Kobe Steel, Ltd. Process for preventing formation of gypsum scale in a flue gas desulfurization process
US4100256A (en) * 1977-03-18 1978-07-11 The Dow Chemical Company Hydrolysis of carbon oxysulfide
US4150096A (en) * 1977-10-31 1979-04-17 Nelms William M Process for treating combustion gases
US4177245A (en) * 1978-05-24 1979-12-04 Battelle Development Corporation Scale suppression in lime and limestone scrubbers
US4310348A (en) * 1978-08-22 1982-01-12 Egyt Gyogyszervegyeszeti Gyar Plant growth regulating compositions
US4216087A (en) * 1978-12-18 1980-08-05 The Dow Chemical Company Scrubber scale prevention
US4388281A (en) * 1980-05-24 1983-06-14 Hoelter Heinz Noxious-component removal from flue gas and compositions useful therefor

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4783327A (en) * 1987-08-13 1988-11-08 The Dow Chemical Company Sulfur dioxide removal from gas streams using hydroxyalkyl substituted piperazinones
US4735787A (en) * 1987-08-17 1988-04-05 Nalco Chemical Company Scale inhibitor for intermittent washed mist eliminators in flue gas desulfurization systems
US4786329A (en) * 1987-09-09 1988-11-22 The Dow Chemical Company Asphalt compositions containing anti-stripping additives prepared from amines or polyamines and phosphonates
US5077023A (en) * 1989-08-01 1991-12-31 Basf Aktiengesellschaft Reduction in the rate of oxidation of sulfite solutions
US5120516A (en) * 1990-01-08 1992-06-09 Physical Sciences, Inc. Process for removing nox emissions from combustion effluents
US5108723A (en) * 1990-08-16 1992-04-28 The Dow Chemical Company Process for absorption of sulfur compounds from fluids
US5098681A (en) * 1990-08-16 1992-03-24 The Dow Chemical Company Process for absorption of sulfur compounds from fluids
US5236678A (en) * 1990-08-16 1993-08-17 The Dow Chemical Company Process for absorption of sulfur compounds from fluids using piperidines
US5342593A (en) * 1990-08-16 1994-08-30 The Dow Chemical Company Process for absorption of sulfur compounds from fluids
US5433934A (en) * 1991-08-13 1995-07-18 The Dow Chemical Company Method for simultaneous absorption of sulfur dioxide and nitric oxide from flue gas
US20130220888A1 (en) * 2012-02-29 2013-08-29 Uop, Llc Process, vessel, and apparatus for removing one or more sulfur compounds
US9303214B2 (en) * 2012-02-29 2016-04-05 Uop Llc Process, vessel, and apparatus for removing one or more sulfur compounds
CN102580504A (zh) * 2012-03-07 2012-07-18 武汉兴能环保技术有限公司 一种新型氨法脱硫吸收装置

Also Published As

Publication number Publication date
AU573617B2 (en) 1988-06-16
JPS6161617A (ja) 1986-03-29
EP0172288B1 (en) 1987-11-11
AU3259784A (en) 1986-03-06
EP0172288A1 (en) 1986-02-26
CA1215822A (en) 1986-12-30
IN161736B (Sortimente) 1988-01-30

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